反応 #43365

反応方程式

2-chloro-1-methylpyridinium iodide

4-Trifluoromethylphenyl isothiocyanate

4-(2-(5-(trifluoromethyl)-1H-imidazol-2-yl)pyridin-4-yloxy)-N1-methylbenzene-1,2-diamine

Triethylamine

→

title compound

収率 61.1%

{1-Methyl-5-[2-(5-trifluoromethyl-1H-imidazol-2-yl)-pyridin-4-yloxy]-1H-benzo-imidazol-2-yl}-(4-trifluoromethyl-phenyl)-amine

収率 61.1%

溶媒

acetonitrile

water

反応条件

後処理

1. 1
   温度The reaction mixture was heated to 50° C. for 5 h
2. 2
   workup.STIRRINGAfter stirring the mixture for 2 h
3. 3
   ろ過the solid was collected by filtration
4. 4
   洗浄washed with 2:1 acetonitrile/water (3×1 mL)

実験手順

4-Trifluoromethylphenyl isothiocyanate (200 mg, 1 mmol) was added to a mixture of 4-(2-(5-(trifluoromethyl)-1H-imidazol-2-yl)pyridin-4-yloxy)-N1-methylbenzene-1,2-diamine (350 mg, 1 mmol) in 3 mL of acetonitrile. After stirring for 20 min at ambient temperature, HPLC analysis showed complete conversion. Triethylamine (0.3 mL, 2.2 mmol) was added followed by 2-chloro-1-methylpyridinium iodide (270 mg, 1.05 mmol). The reaction mixture was heated to 50° C. for 5 h. The heating was stopped and 1.5 mL of water was added. After stirring the mixture for 2 h, the solid was collected by filtration and washed with 2:1 acetonitrile/water (3×1 mL) to afford 317 mg (61%) of the title compound.

出典